共热解法制备方解石/生物炭复合材料及其吸附Pb(II)性能和机制

王申宛; 钟爽; 郑丽丽; 艾斌凌; 校导; 郑晓燕; 杨旸; 盛占武

doi:10.13801/j.cnki.fhclxb.20210309.002

共热解法制备方解石/生物炭复合材料及其吸附Pb(II)性能和机制

doi: 10.13801/j.cnki.fhclxb.20210309.002

王申宛^{1, 2,},
钟爽^1,,
郑丽丽¹,
艾斌凌¹,
校导¹,
郑晓燕¹,
杨旸¹,
盛占武^1, ,

1.
中国热带农业科学院　海口实验站，海口 571101
2.
海南大学　食品科学与工程学院，海口 570228

基金项目: 海南省自然科学基金(319QN267)；中央级公益性科研院所基本科研业务费创新团队专项(17CXTD-05)；海南省重点研发计划(ZDYF2019187)

详细信息

作者简介:
王申宛，硕士生，研究方向为食品加工及副产物综合利用

钟爽，博士，副研究员，研究方向为热带特色作物资源开发与综合利用

通讯作者:
盛占武，博士，研究员，研究方向为农场品加工及副产物综合利用　E-mail：shengzhanwu100@163.com

中图分类号: TB332
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- 被引次数: 0
出版历程
- 收稿日期: 2020-12-14
- 录用日期: 2021-02-25
- 网络出版日期: 2021-03-10
- 刊出日期: 2021-12-01

Preparation of calcite/biochar composite by co-pyrolysis and its adsorption properties and mechanism for Pb(II)

1.
Haikou Experimental Station, Chinese Academy of Tropical Agricultural Sciences, Haikou 571101, China
2.
College of Food Science and Engineering, Hainan University, Haikou 570228, China

摘要

摘要: 为了制备一种高效吸附含Pb(II)废水的生物炭材料，以椰壳(CS)和方解石(CAL)为原料，采用共热解法分别在500℃、600℃、700℃制备了方解石/生物炭(CAL/BC)复合材料。通过SEM、ICP-MS、BET、XRD、FTIR等方法对CAL/BC复合材料的表面微观形态和结构进行了表征。结果发现，三种热解温度条件下，CAL均能够与CS紧密结合，而且CAL/BC具有较大的比表面积，表面含有丰富的官能团。批量吸附实验结果表明，CAL和CS质量比为1∶2，pH值为5.5，吸附剂添加量为1.5 g·L⁻¹，此时CAL/BC复合材料对Pb(II)的吸附量分别为95.24 mg·g⁻¹(500℃)、99.01 mg·g⁻¹(600℃)、185.19 mg·g⁻¹(700℃)，可见热解温度为700℃时，吸附效果最佳。吸附过程符合二级动力学模型和Langmuir等温线模型。CAL/BC复合材料吸附Pb(II)的主要机制是沉淀、离子交换、阳离子-π作用、孔隙填充和静电引力。此外，CAL/BC复合材料在4次吸附-解吸循环后仍能保持较高的Pb(II)去除率。因此，共热解法制备的CAL/BC复合材料在处理废水中的Pb(II)方面具有广阔的应用前景。
- 方解石 /
- 椰壳 /
- 生物炭 /
- 复合材料 /
- Pb(II) /
- 吸附
Abstract: In order to obtain a biochar material which adsorbs PB (II) in wastewater efficiently, calcite/biochar (CAL/BC) composite was prepared by co-pyrolysis at 500℃, 600℃ and 700℃, using coconut shell (CS) and calcite (CAL) as raw materials. The surface morphology and structure of CAL/BC composites were characterized by SEM, ICP-MS, BET, XRD and FTIR. The results show that CAL and CS combine tightly under the three pyrolysis tempera-tures, and CAL/BC has a large specific surface area and a large number of functional groups. The maximum adsorption capacities of PB (II) on CAL/BC composite (CAL∶ CS=1∶ 2, mass ratio) prepared at 500℃, 600℃, and 700℃ are 95.24 mg·g⁻¹, 99.01 mg·g⁻¹, and 185.19 mg·g⁻¹. The optimum adsorption condition is pH=5.5 and the amount of adsorbent is 1.5 g·L⁻¹. The adsorption process conforms to the second-order kinetic model and Langmuir isotherm model. The mechanisms of adsorption of Pb(II) on CAL/BC composites are precipitation, ion exchange, cation-π action, pore filling and electrostatic gravitation. In addition, the removal rate of Pb(II) by CAL/BC composite remains high level after 4 adsorption-desorption cycles. Therefore, the CAL/BC composite prepared by co-pyrolysis has a excellent application prospect in the treatment of Pb(II) in wastewater.
- calcite /
- coconut shell /
- biochar /
- composites /
- Pb(II) /
- adsorption

HTML全文

图 1 方解石(CAL)与椰壳(CS)不同质量比对CAL/生物炭(BC)复合材料吸附Pb(II)性能的影响

Figure 1. Effect of mass ratio of calcite (CAL)∶coconut shell (CS) on Pb(II) adsorption capacity by CAL/biochar (BC) composite

η—Removal rate of Pb(II) by adsorbent

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图 2 不同CAL/BC复合材料添加量Q_e对Pb(II)吸附效果的影响

Figure 2. Effect of CAL/BC dosage on Pb(II) adsorption capacity Q_eby CAL/BC composite

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图 3 pH对CAL/BC复合材料去除Pb(II)的影响 (a) 及不同热解温度条件下制备的CAL/BC复合材料的零电荷点(pH_pzc) (b)

Figure 3. Effect of pH values on Pb(II) removal by CAL/BC composite (a) and point of zero charge (pH_pzc) of CAL/BC composite prepared at different temperatures (b)

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图 4 吸附时间对不同温度条件下制备的CAL/BC复合材料对Pb(II)吸附量的影响的准一级和准二级动力学模型拟合 (a) 和颗粒内扩散模型 (b)

Figure 4. Effect of adsorption time on Pb(II) adsorption capacity by CAL/BC composite prepared at different temperatures and fits of pseudo first-order and pseudo second-order kinetic models (a), intra-particle diffusion model (b)

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图 5 500℃ (a)、600℃ (b)、700℃ (c) 条件下制备的CAL/BC复合材料吸附Pb(II)的Langmuir和Freundlich等温吸附模型拟合

Figure 5. Fitting of Langmuir and Freundlich isotherm models of CAL/BC composite prepared at 500℃ (a), 600℃ (b) and 700℃ (c)

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图 6 CAL、BC和CAL/BC复合材料吸附Pb(II)前后的SEM图像

Figure 6. SEM images of CAL, BC and CAL/BC composite before and after adsorption of Pb(II)

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图 7 不同温度条件下制备的BC、CAL/BC复合材料的XRD图谱 ((a)~(b)) 和FTIR图谱 (c)

Figure 7. XRD patterns ((a)-(b)) and FTIR spectra (c) of BC and CAL/BC composite prepared at different temperatures

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图 8 CAL/BC复合材料吸附Pb(II)前后的FTIR图谱

Figure 8. FTIR spectra of CAL/BC composite before and after Pb(II) adsorption

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图 9 CAL/BC复合材料循环再生后吸附Pb(II)的性能

Figure 9. Adsorption properties of CAL/BC composite for Pb(II) after repeated recycling

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表 1 不同温度下制备的CAL/BC复合材料吸附Pb(II)的动力学参数

Table 1. Kinetic parameters of Pb(II) adsorption by the CAL/BC composite prepared at different temperatures

Temprature/℃	Q_e,exp/(mg·g⁻¹)	Pseudo-first-order			Pseudo-second-order
Temprature/℃	Q_e,exp/(mg·g⁻¹)	k₁/min⁻¹	Q_e,calu/(mg·g⁻¹)	R²	k₂/(g·mg⁻¹·min⁻¹)	Q_e,calu/(mg·g⁻¹)	R²
500	48.1844	3.1670	23.7362	0.9847	0.0035	48.7805	0.9998
600	57.1612	3.1963	24.4419	0.9752	0.0017	57.8035	0.9986
700	64.8022	3.0806	21.7715	0.9151	0.0029	64.9351	0.9999
Note: Q_e,exp—Equilibrium sorption capacity obtained from experiment; k₁—First-order apparent sorption rate constant; Q_e,calu—Equilibrium sorption capacity calculated by pseudo-first order kinetics or pseudo-second order kinetics; k₂—Second-order apparent sorption rate constant; R²—Correlation coefficient.

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表 2 不同温度下制备的CAL/BC复合材料吸附Pb(II)的颗粒内扩散参数

Table 2. Intra-particle diffusion parameters of Pb(II) adsorption by the CAL/BC composite prepared at different temperatures

Temprature/ ℃	Film diffusion			Intra-particle diffusion			Equilibrium stage
Temprature/ ℃	K_p1/ (mg·g⁻¹·min^−0.5)	C₁/ (mg·g⁻¹)	R²	K_p2/ (mg·g⁻¹·min^−0.5)	C₂/ (mg·g⁻¹)	R²	K_p3/ (mg·g⁻¹·min^−0.5)	C₃/ (mg·g⁻¹)	R²
500	3.9312	17.7720	0.9894	1.7142	26.6200	0.9910	0.0043	48.0720	0.9938
600	4.3769	23.3990	0.9932	1.3454	34.6150	0.9987	0.1284	53.7210	0.9845
700	6.8956	24.2800	0.9960	1.4274	45.1810	0.9987	0.1239	61.5500	0.9912
Note：K_p1, K_p2, K_p3—Rate constants at different stages of internal diffusion; C₁, C₂, C₃—Intercept of corresponding concentration.

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表 3 不同温度下制备的CAL/BC复合材料吸附Pb(II)的Langmuir和Freundlich吸附等温线参数

Table 3. Langmuir and Freundlich adsorption isotherm parameters of Pb(II) adsorption by the CAL/BC composite prepared at different temperatures

Adsorption temprature/℃	Temprature/℃	Langmuir			Freundlich
Adsorption temprature/℃	Temprature/℃	Q_max/(mg·g⁻¹)	K_L/(L·mg⁻¹)	R²	1/n	K_F/(mg·g⁻¹)	R²
25	500	95.24	0.0798	0.9831	0.4455	2.7511	0.7557
	600	99.01	0.0728	0.9742	0.4512	2.6437	0.7659
	700	185.19	0.2935	0.9903	0.3461	219.7260	0.9717
30	500	151.52	0.0746	0.9718	0.5204	6.7442	0.9408
	600	123.46	0.1070	0.9913	0.2761	67.4520	0.9672
	700	204.08	0.4153	0.9925	0.4022	328.3842	0.9372
35	500	185.19	0.1949	0.9811	0.4841	70.2934	0.9691
	600	158.73	0.2079	0.9816	0.3882	82.7148	0.9548
	700	222.22	1.3235	0.9941	0.4343	1 150.8854	0.9763
Note: Q_max—Maximum sorption capacity; K_L—Adsorptive constant of Langmuir model; 1/n—Empirical parameter varied with the degree of heterogeneity of adsorbing sites; K_F—Adsorptive constant of Freundlich model.

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表 4 复合前后材料元素含量及BET比表面积

Table 4. Element mass and BET specific surface area of materials before and after composite

Material	Element mass fraction/wt%				S_BET/(m²·g⁻¹)
Material	C	O	Ca	Mg	S_BET/(m²·g⁻¹)
BC500℃	67.44	0	0.26	0.15	5.69
BC600℃	77.45	0	0.10	0.06	103.39
BC700℃	85.48	3.81	0.10	0.04	347.43
CAL	4.54	47.80	22.00	14.58	9.30
CAL/BC500℃	15.81	16.59	18.09	13.82	50.86
CAL/BC600℃	21.12	14.89	17.66	10.43	93.20
CAL/BC700℃	0	15.07	18.03	10.65	285.89
Note: S_BET—BET surface area.

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